HRID2244070

反应详情

EQUATION

反应方程式

HRID 2244070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A solution of 1-amino-4-bromo-6-fluoro-isoquinoline (0.1179 g, 0.49 mmol), and hydrazine (0.5 mL) in THF (5 mL) is microwaved at 100° C. for 40 min. Then it is placed in an oil bath and is stirred at 100° C. for 16 h. The reaction mixture is cooled to RT. It is treated with NaHCO3 (satd. aq, 10 mL). The aqueous phase is extracted with EtOAc (2×). The combined organic layers are washed with brine, and dried over MgSO4. The solvent is evaporated and the residue is dried under vacuum to afford 0.079 g (64%) of 4-Bromo-6-hydrazino-isoquinolin-1-ylamine. LC/MS m/z=254 [M+H]+.

WORKUP

后处理

  1. customThen it is placed in an oil bath
  2. temperatureThe reaction mixture is cooled to RT
  3. extractionThe aqueous phase is extracted with EtOAc (2×)
  4. washThe combined organic layers are washed with brine
  5. dry with materialdried over MgSO4
  6. customThe solvent is evaporated
  7. customthe residue is dried under vacuum